CN101961445A - Method for simultaneously extracting various bioactive components from Chinese yam by using subcritical water as medium - Google Patents

Method for simultaneously extracting various bioactive components from Chinese yam by using subcritical water as medium Download PDF

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Publication number
CN101961445A
CN101961445A CN2010105005003A CN201010500500A CN101961445A CN 101961445 A CN101961445 A CN 101961445A CN 2010105005003 A CN2010105005003 A CN 2010105005003A CN 201010500500 A CN201010500500 A CN 201010500500A CN 101961445 A CN101961445 A CN 101961445A
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China
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chinese yam
rhizoma dioscoreae
extract
allantoin
subcritical water
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CN2010105005003A
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Chinese (zh)
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张连富
张华伟
刘河明
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江南大学
利川市汇川现代农业有限公司
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Priority to CN2010105005003A priority Critical patent/CN101961445A/en
Publication of CN101961445A publication Critical patent/CN101961445A/en

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Abstract

A method for simultaneously extracting various bioactive components from Chinese yam by using the subcritical water extraction technique belongs to the technical field of extracting natural bioactive components. The invention provides a method for simultaneously extracting various bioactive components, such as Chinese yam polysaccharide, dioscin, allantoin, and the like, from Chinese yam by using the subcritical water extraction technique and using the by-products of processing Chinese yam tuber and Chinese yam, such as the Chinese yam skin and/or bulbil, and the like, as the raw materials, wherein the bulbil is the super-thin Chinese yam branches, the irregular Chinese yam tubers, and the like, which are removed from the process of treating Chinese yam. The extracting process comprises the steps of once charging, collecting in steps, and changing the water polarity by adjusting the temperature/pressure of the water under the subcritical state, so as to selectively extract the active components having different polarities in the sample and simultaneously extract various active components. The extracted products can be used for separating and purifying a specific component and also can be directly used as the Chinese yam extractives after being decompressed and concentrated for making medicine, makeup and functional food.

Description

Subcritical water extracts the method for multiple bioactive ingredients in the Rhizoma Dioscoreae simultaneously as medium

Technical field

A kind of method of using the Subcritical Water Extraction technology to extract multiple bioactive ingredients in the Rhizoma Dioscoreae simultaneously.The present invention is with the Rhizoma Dioscoreae tuber, (Bulbilus dioscoreae is meant the meticulous Rhizoma Dioscoreae branch of rejecting in the Rhizoma Dioscoreae processing for by-product that Rhizoma Dioscoreae processing produces such as Rhizoma Dioscoreae skin and/or Bulbilus dioscoreae, the Rhizoma Dioscoreae tuber of shape irregularity etc.) be raw material, utilize the Subcritical Water Extraction technology to extract multiple bioactive ingredients such as Chinese yam polysaccharide in the Rhizoma Dioscoreae simultaneously, dioscin, the method of allantoin etc., once charging in the leaching process, substep is collected, change the polarity of water by the temperature/pressure of adjusting water under the subcritical state, and then show selective extraction to opposed polarity active component in the sample, realize the synchronous exploitation of various active composition.Extract further separation, purification that product can be used for special component, also can behind concentrating under reduced pressure, directly be used for functional food, Cosmetic Manufacture, belong to active skull cap components extractive technique field as Rhizoma Dioscoreae extract.

Background technology

Rhizoma Dioscoreae (Rhizoma Dioscoreae) is the underground tuber of Dioscoreaceae plant Rhizoma Dioscoreae (Dioscorea oppositaThunb), it is a common Chinese medicine material simply, it is again a kind of vegetable, listed in first batch of dietotherapeutic Resource TOC in March, 2002 by Ministry of Public Health, have good biological activity and edible safety.Existing studies show that, contain abundant Chinese yam polysaccharide, allantoin, dioscin isoreactivity composition in the Rhizoma Dioscoreae, have multi-efficiencies such as promoting epithelial growth, antiinflammatory, antibacterial, skin protection, beauty treatment, hair care, hair caring and coordinate plant growth, be widely used in many fields such as functional food, medicine, daily chemicals and agricultural chemicals.

Chinese yam polysaccharide in the Rhizoma Dioscoreae, allantoin, the extraction of dioscin isoreactivity composition mainly contains solvent extraction at present, enzyme is handled the back solvent extraction, the ultrasound wave secondary solvent extracts, the extracting method and the supercritical fluid extraction of aid in treatment means considered in microwave-assisted solvent extraction etc., formed intellectual property also mainly concentrates on the control of solvent extraction condition, enzyme is handled the kind of enzyme in the solvent extraction of back, enzymatic hydrolysis condition, optimization for extracting condition, action of ultrasonic waves intensity when the ultrasound wave secondary solvent extracts, selection of time, the intensity that microwave-assisted is handled, aspects such as selection of time.In essence, the said extracted method all exists and need with an organic solvent, easily cause organic solvent residual in a large number, and batch production, production efficiency are low, and each active component extracts, can not realize the defectives such as seamless connection of extraction process separately.The report of also useful supercritical carbon dioxide extraction Chinese yam polysaccharide and allantoin is (as national inventing patent, application number 200610069598.5, publication number CN1958575a), but in fact supercritical carbon dioxide is more suitable for the extracting apolar chemical compound, to the effect of extracting of polysaccharide, saponins, flavonoid and allantoin isopolarity composition very poor [Jin Hongyun, the applied research of subcritical water and progress, hydrometallurgy, 2005:24 (2), 66-8; Wu Renming, the application of Subcritical Water Extraction in analytical chemistry, chemical progress, 2002:14 (1), 32-6].

The sub-critical flow body technique is infant industry's technology of just having risen and just having arrived at rapid permeability every field the nineties in 20th century.Compare with light water, the density of subcritical water, viscosity and dielectric constant take place sharply to change, have near density of liquid and solvability, the viscosity of similar gas and diffusion coefficient, its dielectric constant (ε) 80 drops to similar methanol, alcoholic acid scope (ε=8~24) under the normal temperature and pressure, and the solvability of polarity, low pole chemical constituent is significantly improved.With subcritical water is environmentally friendly solvent, can change phase behavior, the accelerated solvent effect of extraction system, the heterogeneous reaction that becomes under the conventional solvent condition is homogeneous reaction, increase diffusion coefficient, reduce mass transfer and heat transmission resistance, can in the shorter time, reach extraction equilibrium, shorten the processing time, can also control the distribution of extracting product by the temperature/pressure of regulating and control subcritical system.Therefore, substitute poisonous and hazardous organic solvent commonly used with subcritical water and carry out bioactive ingredients and extract, have that equipment is simple, the extraction time is short, energy expenditure is little, the later separation purification is convenient, can not cause plurality of advantages such as environmental pollution substantially.Simultaneously,, can change the polarity of water, thereby can optionally extract the composition of opposed polarity in the sample, realize once continuous extraction, the substep collection of charging, plurality of target composition by changing extracting pressure/temperature.The Subcritical Water Extraction technology has become the most noticeable technology in food, chemical industry, the herbal development field, is applied to the preparation of food additive, functional factor and the recovery renewable resources of food processing garbage rapidly.

Summary of the invention

The purpose of this invention is to provide a kind of method of utilizing the Subcritical Water Extraction technology to extract multiple bioactive ingredients in the Rhizoma Dioscoreae simultaneously, by-product that produces with the processing of Rhizoma Dioscoreae tuber, Rhizoma Dioscoreae in the practice such as Rhizoma Dioscoreae skin and/or Bulbilus dioscoreae are raw material, utilize the Subcritical Water Extraction technology to extract wherein multiple bioactive ingredients such as Chinese yam polysaccharide, dioscin, allantoin etc. simultaneously.Having raw material need not over grind, in the extraction not with an organic solvent, but bioactive ingredients, raffinate such as the strong continuous extraction Chinese yam polysaccharide/dioscin of extraction selectivity and allantoin can continue characteristics such as innoxious use, both simplify production technology, improved production efficiency again.

Technical scheme of the present invention: be that the by-product that produces of Rhizoma Dioscoreae tuber, the Rhizoma Dioscoreae processing with preliminary fragmentation such as Rhizoma Dioscoreae skin and/or Bulbilus dioscoreae are raw material (0.2~1.0cm X 0.5~1.0cm), with the subcritical water is extractant, under the 505KPa condition, the extraction temperature that progressively raises in 100~260 ℃ of scopes, can obtain Chinese yam polysaccharide, dioscin, allantoin successively is the extract of main active.These extracts can be further purified Chinese yam polysaccharide, dioscin, allantoin wherein again after substep is collected, after also can directly concentrating, use as Rhizoma Dioscoreae extract.

Treatment process

(1) raw material gives processing: take by weighing the Rhizoma Dioscoreae tuber of certain mass, by-product such as Rhizoma Dioscoreae skin and/or the Bulbilus dioscoreae that Rhizoma Dioscoreae processing produces, behind the granule through tentatively being crushed to 0.2~1.0cm X, 0.5~1.0cm size, join in the material basket in the extractor;

(2) preparation of subcritical water: the deionized water that will remove dissolved oxygen is transported to Fast Heating in the preheater, makes deionized water reach subcritical state;

(3) extraction: the subcritical water that temperature is reached setting value is transported in the extractor, regulates the Pressure/Temperature of subcritical water, when the material in the extractor is in the Pressure/Temperature condition of setting, begins to extract:

At pressure is to extract under 505KPa, 100~150 ℃ of conditions of temperature after certain hour, extracting solution begin to flow out, and it is pumped in the cooler cool off, and can collect extract I to room temperature.

Keep extractor pressure 505KPa, the temperature of extractor is brought up to extracted under 150~210 ℃ of conditions after certain hour, extracting solution begin to flow out, it is pumped in the cooler cool off, to room temperature, can collect extract II.

Keep extractor pressure 505KPa, the temperature of extractor is brought up to extracted under 210~260 ℃ of conditions after certain hour, extracting solution begin to flow out, it is pumped in the cooler cool off, to room temperature, can collect extract III.

(4) processing of extract

Extract I, II, III are merged the back concentrating under reduced pressure, can obtain Rhizoma Dioscoreae extract extractum; Also further crushed after being dried obtains the Rhizoma Dioscoreae extract powder, wherein contains bioactive ingredients such as Chinese yam polysaccharide, allantoin, dioscin.

I is evaporated to paste with extract, adds after dehydrated alcohol concentration of alcohol to the mixture reaches 70%, staticly settles 10-12 hour, filters to obtain insoluble matter and drying, pulverizing, can obtain the Chinese yam polysaccharide that purity reaches 60-95%.

(mass ratio is 2~20: 1) mix with active carbon with extract II, after leaving standstill 1~2 hour, low-speed centrifugal separates (300~2000 rev/mins) and dispels moisture, again with washing with alcohol and after isolating active carbon, the concentrating under reduced pressure organic facies, can obtain allantoin, its content can reach 40~80 grams/100 grams.After ethanol or recrystallizing methanol, its purity can further improve 90~95%.

Extract III is evaporated to 1/10 of original volume, last AB28 macroporous adsorptive resins, earlier with behind the deionized water eluting, the ethanol elution of reuse 10%, 20%, 30%, 40% volume fraction, collect 30%, 40% ethanol elution component, be evaporated to driedly, promptly get the dioscin powder, its purity is 40~80%.

Beneficial effect of the present invention

The present invention can need not or significantly reduce under the condition of consumption of organic solvent, and once 3 kinds of main functional components in the Rhizoma Dioscoreae are extracted in charging simultaneously; According to the market demand, can produce 4 kinds of products, both improved the operating efficiency of extraction, reduced the energy expenditure in the extraction process again, also make extracting operation that the pollution of environment is reduced to bottom line simultaneously, economical, societal benefits are remarkable.

The specific embodiment

Embodiment 1

(1) raw material gives processing: take by weighing the Rhizoma Dioscoreae skin removed in the Rhizoma Dioscoreae processing (account for Rhizoma Dioscoreae treating capacity 25~30%) 1000 grams, tentatively be crushed to the granule of 0.2~1.0cm X, 0.5~1.0cm size after, join in the material basket in the extractor;

(2) preparation of subcritical water: the deionized water that will remove dissolved oxygen is transported to Fast Heating in the preheater, makes deionized water reach subcritical state;

(3) extraction: the subcritical water that temperature is reached setting value is transported in the extractor, regulate the Pressure/Temperature of subcritical water, when the material pressure in the extractor reaches 505KPa, in 30 minutes, progressively extraction temperature is increased to 260 ℃ from 100, collect extracting solution, concentrating under reduced pressure after the cooler cooling can obtain Rhizoma Dioscoreae and extract extractum; Also can further carry out drying and pulverizing, obtain Rhizoma Dioscoreae extract powder 38.6 grams, wherein contain bioactive ingredients such as Chinese yam polysaccharide, allantoin, dioscin.

Embodiment 2

(1) raw material gives processing: take by weighing Rhizoma Dioscoreae tuber 1000 grams, behind the granule through tentatively being crushed to 0.2~1.0cm X, 0.5~1.0cm size, join in the material basket in the extractor;

(2) preparation of subcritical water: the deionized water that will remove dissolved oxygen is transported to Fast Heating in the preheater, makes deionized water reach subcritical state;

(3) extraction: setting extractor pressure is under 505KPa, the input subcritical water is also adjusted the extractor temperature, in 15 minutes the temperature of extractor being improved 150 ℃ gradually from 100 ℃ extracts, after extracting solution begins to flow out, it is pumped in the cooler cool off, to room temperature, can collect extract I.

Keep extractor pressure 505KPa, in 10 minutes, the temperature of extractor is brought up to 210 ℃ gradually from 150 ℃ and extract, after extracting solution begins to flow out, it is pumped in the cooler cool off, to room temperature, can collect extract II.

Keep extractor pressure 505KPa, in 10 minutes, the extractor temperature is brought up to 260 ℃ since 210 ℃ and extract, after extracting solution flows out, it pumped in the cooler cool off, to room temperature, can collect extract III.

(4) processing of extract:

I is evaporated to paste with extract, adds after dehydrated alcohol concentration of alcohol to the mixture reaches 70%, staticly settles 10 hours, filters to obtain insoluble matter and drying, pulverizing, can obtain purity and reach 60~95% Chinese yam polysaccharide 18.2 grams.

With extract II and active carbon (mass ratio is 2~20: 1) mix, leave standstill 1 hour after, low-speed centrifugal separates (300~2000 rev/mins) and dispels moisture, again with washing with alcohol and after isolating active carbon, the concentrating under reduced pressure organic facies can obtain allantoin, and its content can reach 40~60 grams/100 grams.After ethanol or recrystallizing methanol, its purity can further improve 90~95%.

Extract III is evaporated to 1/10 of original volume, last AB28 macroporous adsorptive resins, earlier with behind the deionized water eluting, the ethanol elution of reuse 10%, 20%, 30%, 40% volume fraction, collect 30%, 40% ethanol elution component, be evaporated to driedly, promptly get dioscin powder 9.3 gram, its purity is 42.5%.

Embodiment 3

(1) raw material gives processing: take by weighing Bulbilus dioscoreae 1000 grams that Rhizoma Dioscoreae processing produces, behind the granule through tentatively being crushed to 0.2~1.0cm X, 0.5~1.0cm size, join in the material basket in the extractor;

(2) preparation of subcritical water: the deionized water that will remove dissolved oxygen is transported to Fast Heating in the preheater, makes deionized water reach subcritical state;

(3) extraction: setting extractor pressure is under 505KPa, the input subcritical water is also adjusted the extractor temperature, in 15 minutes the temperature of extractor being improved 140 ℃ gradually from 100 ℃ extracts, after extracting solution begins to flow out, it is pumped in the cooler cool off, to room temperature, can collect extract I.

Keep extractor pressure 505KPa, in 20 minutes, the temperature of extractor is brought up to 210 ℃ gradually from 140 ℃ and extract, after extracting solution begins to flow out, it is pumped in the cooler cool off, to room temperature, can collect extract II.

Keep extractor pressure 505KPa, in 18 minutes, the extractor temperature is brought up to 260 ℃ since 210 ℃ and extract, after extracting solution flows out, it pumped in the cooler cool off, to room temperature, can collect extract III.

(4) processing of extract:

I is evaporated to paste with extract, adds after dehydrated alcohol concentration of alcohol to the mixture reaches 70%, staticly settles 12 hours, filter obtain insoluble matter and through repeat to purify, dry, pulverize, can obtain purity and reach 95% Chinese yam polysaccharide 8.3 grams.

With extract II and active carbon (mass ratio is 2~20: 1) mix, leave standstill 1 hour after, low-speed centrifugal separates (300~2000 rev/mins) and dispels moisture, again with washing with alcohol and after isolating active carbon, the concentrating under reduced pressure organic facies can obtain allantoin, and its content can reach 52 grams/100 grams.After ethanol or recrystallizing methanol, its purity can further improve 90%.

Extract III is evaporated to 1/10 of original volume, last AB28 macroporous adsorptive resins, earlier with behind the deionized water eluting, the ethanol elution of reuse 10%, 20%, 30%, 40% volume fraction, collect 30%, 40% ethanol elution component, be evaporated to driedly, promptly get dioscin powder 11.2 gram, its purity is 63.6%.

Claims (7)

1. method of using the Subcritical Water Extraction technology to extract multiple bioactive ingredients in the Rhizoma Dioscoreae simultaneously, it is characterized in that the by-product that produces with the processing of Rhizoma Dioscoreae tuber, Rhizoma Dioscoreae such as Rhizoma Dioscoreae skin and/or Bulbilus dioscoreae (Bulbilus dioscoreae is meant the meticulous Rhizoma Dioscoreae branch of rejecting in the Rhizoma Dioscoreae processing, the Rhizoma Dioscoreae tuber of shape irregularity etc.) are raw material, utilize the Subcritical Water Extraction technology to extract the method for multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin etc. simultaneously.The extract that is obtained can carry out further purification respectively, also can directly use behind concentrating under reduced pressure.
2. extract the method for multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin simultaneously based on the usefulness Subcritical Water Extraction technology of claim 1, it is characterized in that using a kind of in Rhizoma Dioscoreae tuber, Rhizoma Dioscoreae processing byproduct and/or the Bulbilus dioscoreae or use simultaneously wherein two or three as extraction feed.
3. method of using the Subcritical Water Extraction technology to extract multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin etc. simultaneously, it is characterized in that raw material is carried out preliminary fragmentation, its size is between 0.2~1.0cm X, 0.5~1.0cm, with the subcritical water is extractant, under the 505KPa condition, extract above-mentioned three kinds of active component 100~260 ℃ of scopes.
4. the usefulness Subcritical Water Extraction technology based on claim 3 is extracted the method for multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin simultaneously, it is characterized in that the collection extract that to distribute, also can not add to distinguish to merge and collect extract.
5. the usefulness Subcritical Water Extraction technology based on claim 3 is extracted the method for multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin simultaneously, it is characterized in that the extract that is rich in Chinese yam polysaccharide is evaporated to paste earlier, add again after dehydrated alcohol concentration of alcohol to the mixture reaches 70%, staticly settled 10-12 hour, insoluble matter that filtration at last obtains and drying, pulverizing are to obtain highly purified Chinese yam polysaccharide.
6. the usefulness Subcritical Water Extraction technology based on claim 3 is extracted the method for multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin simultaneously, (mass ratio is 2~20: 1) mix with active carbon to it is characterized in that will being rich in earlier the extract II of allantoin, after leaving standstill 1~2 hour, low-speed centrifugal separates (300~2000 rev/mins) and dispels moisture, with washing with alcohol and after isolating active carbon, the concentrating under reduced pressure organic facies is to obtain allantoin again.
7. the usefulness Subcritical Water Extraction technology based on claim 3 is extracted the method for multiple bioactive ingredients in the Rhizoma Dioscoreae such as Chinese yam polysaccharide, dioscin, allantoin simultaneously, it is characterized in that the extract that will be rich in dioscin earlier is evaporated to 1/10 of original volume, last AB28 macroporous adsorptive resins, earlier with behind the deionized water eluting, the ethanol elution of reuse 10%, 20%, 30%, 40% volume fraction, collect 30%, 40% ethanol elution component, be evaporated to and do to obtain the dioscin powder.
CN2010105005003A 2010-10-09 2010-10-09 Method for simultaneously extracting various bioactive components from Chinese yam by using subcritical water as medium CN101961445A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102599321A (en) * 2012-03-17 2012-07-25 汕头市天悦轻工技术科技有限公司 Manufacturing method for crystallized fruit
CN102702375A (en) * 2012-05-16 2012-10-03 沈阳化工大学 Method for extracting polysaccharide from processed residua of taxus chinensis
CN103356749A (en) * 2013-07-19 2013-10-23 苏州市天灵中药饮片有限公司 Subcritical water extraction process of shuanghuanglian
CN104707356A (en) * 2013-12-14 2015-06-17 河南省亚临界生物技术有限公司 Method used for extracting biological ingredients with sub-critical ethanol solvent
CN107854598A (en) * 2017-11-17 2018-03-30 贵州浩诚药业有限公司 A kind of Baizhi dehumidizer made from gloden cyllress and cape jasmine etc. Chinese herbal medicines and preparation method thereof
CN108239136A (en) * 2016-12-26 2018-07-03 天津延生园生物科技有限公司 A kind of extracting method of dioscin

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《中药材》 20090430 陈赟等 亚临界水萃取技术及其在天然产物分析中的应用 636-638 1-7 第32卷, 第4期 2 *
《环境分析化学》 20090131 但德忠主编 第八节 亚临界水萃取 , *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102599321A (en) * 2012-03-17 2012-07-25 汕头市天悦轻工技术科技有限公司 Manufacturing method for crystallized fruit
CN102702375A (en) * 2012-05-16 2012-10-03 沈阳化工大学 Method for extracting polysaccharide from processed residua of taxus chinensis
CN103356749A (en) * 2013-07-19 2013-10-23 苏州市天灵中药饮片有限公司 Subcritical water extraction process of shuanghuanglian
CN104707356A (en) * 2013-12-14 2015-06-17 河南省亚临界生物技术有限公司 Method used for extracting biological ingredients with sub-critical ethanol solvent
CN108239136A (en) * 2016-12-26 2018-07-03 天津延生园生物科技有限公司 A kind of extracting method of dioscin
CN107854598A (en) * 2017-11-17 2018-03-30 贵州浩诚药业有限公司 A kind of Baizhi dehumidizer made from gloden cyllress and cape jasmine etc. Chinese herbal medicines and preparation method thereof

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